CN110240126B - Tin diselenide with nanoflower structure and preparation method thereof - Google Patents
Tin diselenide with nanoflower structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses tin diselenide with a nanoflower structure and a preparation method thereof, wherein the tin diselenide is a flower-shaped structure with stacked sheet layers, and a microscopic picture of the flower-shaped structure shows that each sheet layer generates other tiny sheet layers, so that the specific surface area of the formed flower-shaped structure is larger; the preparation method of the tin diselenide with the nanoflower structure is simple in process, the used raw materials and the used solvent are free of pollution, and the flower-shaped tin diselenide prepared by selecting the raw materials and selecting the solvent is high in purity, uniform in size and consistent in shape.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of inorganic compound semiconductor nano materials, and particularly relates to tin diselenide with a nanoflower structure and a preparation method thereof.
[ background of the invention ]
In recent years, the unique layered structure of tin diselenide has attracted much attention. The layered structure of the material causes strong phonon scattering between layers, so that the material has low lattice thermal conductivity and anisotropic electronic and photoelectric properties, has wide application prospect in the fields of thermoelectric materials, photoelectric sensing, energy storage materials and the like, and can be applied to solid-phase media of holograms, thermoelectric refrigeration materials, infrared photoelectric instruments, thin-film electrodes, memory change-over switches and the like. At present, the synthesis of tin diselenide nano materials mainly adopts a high-temperature high-pressure method, the synthesis process is complex, the synthesis methods of polycrystalline nano materials comprise physical vapor deposition, a sol-gel method and the like, most of the methods have long preparation process period and high toxicity, and the phase composition is impure. Therefore, it is necessary to research and explore a method for effectively synthesizing tin diselenide nano-structure, which has simple operation, low cost and easy popularization.
The tin diselenide prepared by the method is usually tin diselenide with a sheet or needle structure, and the specific surface area of the tin diselenide with the sheet or needle structure is small, so that the function of the tin diselenide is limited in the practical application process in the fields of sensors, catalysts and the like.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides tin diselenide with a nanoflower structure and a preparation method thereof; the method has the advantages of simple preparation process, safe operation process and no pollution, and the prepared stannum diselenide popcorn has a single-phase powder structure, large specific surface area and uniform shape and size.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the tin diselenide with the nanoflower structure is formed by spirally stacking a plurality of sheet layers, and each sheet layer is formed by spirally stacking and growing crystals; the diameter of tin diselenide formed by spirally stacking a plurality of sheet layers is 1-2 mu m, and the thickness of each sheet layer is 5-10 nm.
The invention is further improved in that:
preferably, the tin diselenide is in a single-phase powder structure.
A preparation method of tin diselenide with a nanoflower structure comprises the following steps:
step 1, heating oleylamine, adding selenium dioxide into the oleylamine, uniformly stirring, adding stannous chloride and n-dodecyl mercaptan, and uniformly stirring to obtain a mixed solution;
step 2, reacting the mixed solution obtained in the step 1 in a sealed environment;
and 3, after the reaction is finished, centrifugally collecting a precipitate, washing the precipitate, and drying the washed precipitate to obtain the tin diselenide with the nanoflower structure.
Preferably, in the step 1, the heating temperature of the oleylamine is 65-75 ℃.
Preferably, in step 1, the molar ratio of the stannous chloride to the selenium dioxide is 1: 1.
Preferably, in step 1, the ratio of selenium dioxide to n-dodecyl mercaptan added is 1 mmol: (0.8-1.2) mL.
Preferably, in step 1, the ratio of selenium dioxide to n-dodecyl mercaptan added is 1 mmol: 1 mL.
Preferably, in the step 2, the reaction temperature is 170-190 ℃ and the reaction time is 24-48 h.
Preferably, in step 3, the washing liquid for washing the precipitated product is a mixed liquid of toluene and ethanol.
Preferably, in the step 3, the drying temperature of the washed precipitate is 50-60 ℃, and the drying time is 4-6 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses tin diselenide with a nanoflower structure, wherein the tin diselenide is a flower-shaped structure with stacked sheet layers, and a microscopic picture of the flower-shaped structure shows that each sheet layer is provided with other tiny sheet layers, so that the specific surface area of the formed flower-shaped structure is larger, and when the tin diselenide is applied to the field of sensors, the adsorption efficiency is high, and the response time is short; when the tin diselenide is used as a catalyst, the catalytic efficiency can be improved.
Furthermore, the tin diselenide is of a powder structure, and each nanoflower structure is uniform in shape, size and dimension, so that the service performance of the material is enhanced.
The invention also discloses a preparation method of tin diselenide with a nanoflower structure, which comprises the steps of heating oleylamine, adding selenium dioxide into the heated oleylamine, and uniformly stirring to ensure that the selenium dioxide can be fully dissolved in the heated oleylamine, wherein the selenium dioxide forms simple substance selenium in the stirring process due to the reducibility of the oleylamine; and adding stannous chloride and n-dodecyl mercaptan, wherein in the reaction process under a closed environment, stannous ions brought in after the stannous chloride is added are combined with elemental selenium to generate hexagonal flaky tin diselenide, the flaky tin diselenide starts to disperse along with the reaction, a plurality of steps driven by screw dislocation to grow are generated on the upper surface and the lower surface, and a flower-shaped structure similar to the stacking of the layers is formed along with the processes of the alternate growth and the spiral rising of the steps. The preparation method has the advantages of simple process, no pollution of used raw materials and solvents, large specific surface area, high purity, uniform size and consistent shape of the prepared flower-shaped tin diselenide through selection of the raw materials and selection of the solvents.
Furthermore, oleylamine is selected as a solvent and a reducing agent, and the heated oleylamine can promote the dissolution of selenium dioxide, so that selenium dioxide firstly generates selenium ions through reduction; on the other hand, as the surfactant, the oleylamine can be combined with the nanoparticles due to the existence of amino groups in the oleylamine, so that the nanoparticles are prevented from agglomerating, and the flower-like nanostructure formed is small and uniform in size.
Furthermore, stannous chloride and stannic oxide are selected as reaction raw materials, so that the purity of the prepared product can be improved, and the flaky stacked flower-shaped tin diselenide is formed.
Furthermore, n-dodecyl mercaptan is added as a reducing agent to promote selenium ions to generate elemental selenium.
[ description of the drawings ]
FIG. 1 is a schematic flow diagram of the overall manufacturing process;
FIG. 2 is a SEM topography of elemental selenium during the preparation of example 1;
FIG. 3 is a low SEM topography picture of tin diselenide produced on a selenium rod during preparation of example 1;
FIG. 4 is a high power SEM morphology picture of tin diselenide flakes during the preparation of example 1;
FIG. 5 is an XRD pattern of the product tin diselenide prepared in example 1;
FIG. 6 is a low-magnification SEM morphology picture of a product tin diselenide prepared in example 1;
FIG. 7 is a high power SEM topography picture of the product tin diselenide prepared in example 1;
FIG. 8 is a high power SEM topography of the product flake tin diselenide prepared in example 1;
FIG. 9 is a high power SEM morphology picture of flaky tin diselenide grown by stacking products prepared in example 1;
fig. 10 is a high resolution transmission electron micrograph of the product tin diselenide prepared in example 1.
[ detailed description ] embodiments
The invention is further described in detail with reference to the accompanying drawings and specific examples, and discloses tin diselenide with a nanoflower structure and a preparation method thereof, wherein the method specifically comprises the following steps:
step 1, mixing reaction raw materials;
heating oleylamine serving as a solvent to 65-75 ℃ in a heat collection type magnetic stirrer, adding selenium dioxide, stirring to obtain a clear solution, and then adding stannous chloride, wherein the molar ratio of the added stannous chloride to the added selenium dioxide is 1: 1; adding n-dodecyl mercaptan to promote the reduction of the selenium dioxide, uniformly stirring to obtain a mixed solution, adding 0.8-1.2 mL of n-dodecyl mercaptan into 1mmol of selenium dioxide, and preferably adding 1mL of n-dodecyl mercaptan into 1mmol of selenium dioxide; in this step, the total volume of oleylamine and n-dodecylmercaptan was 70% of the volume of the reaction vessel.
Step 2, reaction is carried out;
and (3) putting the uniformly stirred mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing and putting the kettle into a constant-temperature oven, heating to 170-190 ℃, and preserving heat for 24-48 h, wherein the preferable heat preservation time is 36 h.
Step 3, working up the reaction product
Taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifuging to collect precipitates, repeatedly centrifuging and washing for 3-5 times by using a toluene/ethanol mixed solution, wherein the volume ratio of toluene to ethanol in the toluene/ethanol mixed solution is 1: 2; and (3) preserving the heat of the washed centrifugal precipitate for 4-6 hours in a vacuum oven at 50-60 ℃ until the centrifugal precipitate is completely dried, so as to obtain the tin diselenide popcorn structure material.
Referring to fig. 1, it can be seen from the flowchart of the method for preparing the structure of tin diselenide nanoflowers that selenium dioxide is added into oleylamine in the above reaction process, selenium ions are formed due to the reducibility of oleylamine after the selenium dioxide is completely dissolved, and then the solution turns into dark red immediately after stannous chloride and n-dodecyl mercaptan are added, which indicates that elemental selenium is generated; in the reaction kettle, with the reaction, stannous chloride is added, and then divalent tin ions brought in are combined with elemental selenium to generate hexagonal flaky tin diselenide; with the progress of the reaction, the flaky tin diselenide begins to disperse, because of the existence of crystal defects, a plurality of steps which are driven by screw dislocation to grow are generated on the upper surface and the lower surface of the flaky tin diselenide, and with the processes of the interpenetration growth and the spiral rising of the steps, a flower-shaped structure which seems to be stacked by sheets is formed finally.
The nanoflower structure of the tin diselenide prepared by the method is a single-phase powder in a macroscopic view, and is uniform in shape and size; microcosmically, the flower-shaped structures are stacked in spiral sheet shapes, the diameter of each flower-shaped structure is 1-2 mu m, and the thickness of a sheet layer on the surface is about 5-10 nm; the structure has the advantages of large specific surface area, simple preparation process, safe operation process and no pollution, so that the prepared tin diselenide with the nanoflower structure and the preparation method have very wide application prospects.
Example 1
Heating 68mL of oleylamine in a heat collection magnetic stirrer to 70 ℃, adding 2.4mmol of selenium dioxide, stirring to obtain a clear solution, adding 2.4mmol of stannous chloride, adding 2.5mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing, putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 180 ℃, preserving the temperature for 36h, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 4 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation in a vacuum oven at 60 ℃ for 6h to obtain the nano tin diselenide material.
XRD, SEM and TEM analyses of the tin diselenide obtained in example 1 and the final product of tin diselenide nanoflower material are shown in FIGS. 2-10.
FIG. 2 is an SEM image of elemental selenium during the preparation process of example 1, and it can be seen that the prepared elemental selenium has a rod-like structure;
FIG. 3 is a SEM image of tin diselenide in low magnification during the preparation process of example 1, from which it can be seen that tin diselenide formed on the surface of the selenium rod has a sheet-like structure;
FIG. 4 is a high SEM topography of tin diselenide during the preparation of example 1, from which it can be seen that the tin diselenide sheet structure is after the selenium rod is consumed;
FIG. 5 is an XRD pattern of a tin diselenide popcorn material prepared in example 1 of the present invention, showing that the material is pure tin diselenide (JCPDS No. 89-2939).
Fig. 6 is a low-power SEM photograph of the tin diselenide popcorn material prepared in example 1 of the present invention, which shows that the prepared tin diselenide nanostructures are all flower-like structures and uniform in size.
Fig. 7 is a high power SEM photograph of the tin diselenide popcorn material prepared in example 1 of the present invention, showing a single tin diselenide popcorn structure, similar to a flower-like structure formed by close packed assembly of nanosheets;
fig. 8 and 9 are high-power SEM morphology pictures of the initial stage of flower-like formation of tin diselenide prepared as a product in example 1, and it can be seen that many small steps exist on the surface of the flaky tin diselenide, so that a nanoflower structure is finally formed.
Fig. 10 is a high resolution transmission electron micrograph of tin diselenide nanoflower material prepared in accordance with example 1 of the present invention, in which the pitch of the stripes corresponds to the (101) interplanar spacing of tin diselenide.
Example 2
Heating 68mL of oleylamine in a heat collection magnetic stirrer to 70 ℃, adding 0.8mmol of selenium dioxide, stirring to obtain a clear solution, adding 0.8mmol of stannous chloride, adding 0.8mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing, putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 180 ℃, preserving the temperature for 24 hours, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 4 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation for 6 hours at 60 ℃ in a vacuum oven to obtain the nano tin diselenide material.
Example 3
Heating 68mL of oleylamine in a heat collection magnetic stirrer to 70 ℃, adding 1.6mmol of selenium dioxide, stirring to obtain a clear solution, adding 1.6mmol of stannous chloride, adding 1.6mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing and putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 180 ℃, preserving the temperature for 48 hours, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 4 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation for 6 hours at 60 ℃ in a vacuum oven to obtain the nano tin diselenide material.
Example 4
Heating 68mL of oleylamine in a heat collection type magnetic stirrer to 68 ℃, adding 1.6mmol of selenium dioxide, stirring to obtain a clear solution, adding 1.6mmol of stannous chloride, adding 1.45mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing, putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 185 ℃, preserving the temperature for 30h, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 4 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation for 5h at 50 ℃ in a vacuum oven to obtain the nano tin diselenide material.
Example 5
Heating 68mL of oleylamine in a heat collection magnetic stirrer to 72 ℃, adding 1.6mmol of selenium dioxide, stirring to obtain a clear solution, adding 1.6mmol of stannous chloride, adding 1.8mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing, putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 175 ℃, preserving the temperature for 24 hours, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 3 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation for 5 hours at 55 ℃ in a vacuum oven to obtain the nano tin diselenide material.
Example 6
Heating 68mL of oleylamine in a heat collection type magnetic stirrer to 65 ℃, adding 1.6mmol of selenium dioxide, stirring to obtain a clear solution, adding 1.6mmol of stannous chloride, adding 1.9mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing and putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 170 ℃, preserving the temperature for 24 hours, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 4 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation for 5 hours at 52 ℃ in a vacuum oven to obtain the nano tin diselenide material.
Example 7
Heating 68mL of oleylamine in a heat collection magnetic stirrer to 75 ℃, adding 1.6mmol of selenium dioxide, stirring to obtain a clear solution, adding 1.6mmol of stannous chloride, adding 1.3mL of n-dodecyl mercaptan, stirring until the selenium dioxide is completely dissolved, immediately putting the mixed solution into a stainless steel high-pressure reaction kettle with a lining of 100mL of polytetrafluoroethylene, sealing, putting the stainless steel high-pressure reaction kettle into a constant-temperature oven, heating to 190 ℃, preserving heat for 40 hours, taking out the reaction kettle after the reaction is finished, naturally cooling to room temperature, centrifugally collecting precipitates, repeatedly centrifugally washing for 5 times by using a methylbenzene/ethanol mixed solution, and drying the precipitates obtained after centrifugation for 5 hours in a vacuum oven at 57 ℃ to obtain the nano tin diselenide material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. Tin diselenide with a nanoflower structure, wherein the tin diselenide with the nanoflower structure is formed by spirally stacking a plurality of sheet layers, and each sheet layer is formed by growing a crystal spiral stack; the diameter of each flower-shaped structure of tin diselenide formed by spirally stacking a plurality of sheet layers is 1-2 mu m, and the thickness of each sheet layer is 5-10 nm;
the tin diselenide is of a single-phase powder structure.
2. A preparation method of tin diselenide with a nanoflower structure is characterized by comprising the following steps:
step 1, heating oleylamine, adding selenium dioxide into the oleylamine, uniformly stirring, adding stannous chloride and n-dodecyl mercaptan, and uniformly stirring to obtain a mixed solution; in step 1, the ratio of the added selenium dioxide to the n-dodecyl mercaptan is 1 mmol: (0.8-1.2) mL;
step 2, reacting the mixed solution obtained in the step 1 in a sealed environment;
step 3, after the reaction is finished, centrifugally collecting a precipitation product, washing the precipitation product, and drying the washed precipitation product to obtain tin diselenide with a nanoflower structure;
stannous chloride adds the back bivalent tin ion of bringing and can combine with simple substance selenium, generates the flaky tin diselenide of hexagon, and along with the going on of reaction, flaky tin diselenide begins the dispersion to can produce the step that a plurality of screw dislocation drive were grown about the top and bottom, along with the process that interlude growth, spiral rising of step, form the accumulational flower column structure of lamella at last.
3. The method for preparing tin diselenide with a nanoflower structure according to claim 2, wherein in the step 1, the heating temperature of oleylamine is 65-75 ℃.
4. The method for preparing tin diselenide with a nanoflower structure according to claim 2, wherein the molar ratio of stannous chloride to selenium dioxide added in step 1 is 1: 1.
5. The method for preparing tin diselenide with a nanoflower structure according to claim 2, wherein in the step 1, the ratio of the added selenium dioxide to the added n-dodecanethiol is 1 mmol: 1 mL.
6. The method for preparing tin diselenide with a nanoflower structure according to claim 2, wherein in the step 2, the reaction temperature is 170-190 ℃ and the reaction time is 24-48 hours.
7. The method for preparing tin diselenide with a nanoflower structure as claimed in claim 2, wherein in step 3, the washing solution for washing the precipitated product is a mixture of toluene and ethanol.
8. The method for preparing tin diselenide with a nanoflower structure according to any one of claims 2 to 7, wherein in the step 3, the drying temperature of the washed precipitate is 50-60 ℃ and the drying time is 4-6 hours.
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